CN106946248A - A kind of method of new transfer graphene film and the preparation method of sensor - Google Patents
A kind of method of new transfer graphene film and the preparation method of sensor Download PDFInfo
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- CN106946248A CN106946248A CN201710265007.XA CN201710265007A CN106946248A CN 106946248 A CN106946248 A CN 106946248A CN 201710265007 A CN201710265007 A CN 201710265007A CN 106946248 A CN106946248 A CN 106946248A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
- G01D5/00—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable
- G01D5/12—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable using electric or magnetic means
- G01D5/14—Mechanical means for transferring the output of a sensing member; Means for converting the output of a sensing member to another variable where the form or nature of the sensing member does not constrain the means for converting; Transducers not specially adapted for a specific variable using electric or magnetic means influencing the magnitude of a current or voltage
Abstract
A kind of method of new transfer graphene film and the preparation method of sensor, are related to technical field of graphene.The method of new transfer graphene film, including:The paraffin of fusing is set to be covered in the graphene film surface for being formed at growth substrates surface.After after paraffin solidification, remove growth substrates and obtain paraffin/graphene composite film, paraffin/graphene composite film is placed in the surface of target substrate, to target substrate heating until paraffin is fitted in target substrate, paraffin is removed using solvent.This method, as new transfer medium, is easy to operation, and can realize and shift graphene film essentially without losses using paraffin.The preparation method of sensor includes:Channel electrode is made on graphene film surface made from the above method, graphene film is made to the pattern of touch sensing, deaeration processing is carried out after graphene film surface laminating optical cement.The graphene film obtained using the above method is complete, substantially lossless and area is big, the making available for sensor.
Description
Technical field
The present invention relates to technical field of graphene, and the more particularly to a kind of method and biography of new transfer graphene film
The preparation method of sensor.
Background technology
Graphene be carbon atom by hexagonal structure it is tightly packed into monoatomic layer two dimensional crystal, graphene has high
The excellent properties such as carrier mobility, high light transmittance, high intensity, it has huge application value in electronic device.In order to
Graphene electronic device is prepared, large scale, the graphene film with superior electrical performance must be made first, and be transferred to properly
Target substrate on.The transfer techniques of graphene film are the key factors for restricting graphene film development.
At present, transfer graphene film is mainly by PMMA methods, resin transfer method or heat release adhesive tape method, but deposits
In certain operation difficulty or inherent shortcoming.Because PMMA is difficult to dissolve when PMMA methods shift graphene, PMMA can only be reduced thick
Degree, is so extremely easily destroyed PMMA films in operation, so as to destroy graphene, and during PMMA transfer graphenes, picks up
The action of PMMA films extremely easily causes PMMA film folds, influences the transfer effect of graphene film.Resin transfer method is consolidated
Some defects can not be removed as the resin bed of transfer material, and sign to graphene and application are all lacking of being difficult to overcome
Point.During heat release adhesive tape method transfer graphene, substrate glue when reaching blowing temperature, have larger power by graphene film from
Substrate surface is peeled off, and this process can destroy the structure of graphene, while also having the residual of glue.
The content of the invention
It is an object of the invention to provide a kind of method of new transfer graphene film, this method is using paraffin as new
Transfer medium, be easy to operation, and can cause shift the basic not damaged of graphene film, integrality it is preferable.
Another object of the present invention is to provide a kind of preparation method of sensor, the graphene obtained using the above method
Film is complete, basic not damaged and area big, the making available for sensor.
The present invention is solved its technical problem and realized using following technical scheme.
The present invention proposes a kind of method of new transfer graphene film, including:
The paraffin of fusing is set to be covered in the graphene film surface for being formed at growth substrates surface.After after paraffin solidification, go
Except growth substrates obtain paraffin/graphene composite film, paraffin/graphene composite film is placed in the surface of target substrate, it is right
Target substrate heating is fitted in target substrate up to paraffin, uses solvent to remove paraffin.
The present invention also proposes a kind of preparation method of sensor, including:On graphene film surface made from the above method
Channel electrode is made, graphene film is made to the pattern of touch sensing, light of being fitted on the graphene film surface of patterning
Learn glue encapsulation and then carry out deaeration processing.
The beneficial effect of the embodiment of the present invention is:In a kind of method of new transfer graphene film, paraffin is used as transfer
Medium, dissolves paraffin, it is possible to achieve shift graphene film essentially without losses by heating melt paraffin and solvent.On the one hand,
It is liquid that paraffin, which is covered in graphene film surface,;It is molten by solvent when on the other hand, by paraffin disengaging graphene film
Take off, during the entire process of transfer graphene film, be used to peel off paraffin and graphene without direct active force, and
The pattern of graphene film is intactly replicated, the basic not damaged transfer of graphene film is realized.Meanwhile, paraffin has low
The characteristics of temperature is melted and be water insoluble, reduces the operation difficulty of graphene film transfer, is conducive to determining growth substrates
Remove technique.And paraffin is cheap, cost reduce further.
A kind of preparation method of sensor, is that graphene is to gather around using made from graphene film made from the above method
There are the superpower what is said or talked about compound of alveolate texture, flexible and, the graphene film that using the above method obtains more further conductive than silicon
Completely, basic not damaged and area are big, therefore the graphene film is used for the making of sensor can to produce sensor stronger
Electric signal.
Brief description of the drawings
Technical scheme in order to illustrate more clearly the embodiments of the present invention, below will be attached to what is used needed for embodiment
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, therefore is not construed as pair
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other related accompanying drawings.
Fig. 1 is the process flow diagram of the method for the new transfer graphene film of the specific embodiment of the invention.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, are the conventional production that can be obtained by commercially available purchase
Product.
Below to the method and the preparation method of sensor of a kind of new transfer graphene film of the embodiment of the present invention
It is specifically described.
A kind of method of new transfer graphene film, including:
The paraffin of fusing is set to be covered in the graphene film surface for being formed at growth substrates surface.After after paraffin solidification, go
Except growth substrates obtain paraffin/graphene composite film, paraffin/graphene composite film is placed in the surface of target substrate, it is right
Target substrate heating is fitted in target substrate up to paraffin, uses solvent to remove paraffin.
Paraffin dissolves paraffin, it is possible to achieve substantially lossless transfer as transfer medium by heating melt paraffin and solvent
Graphene film.Because it is liquid that paraffin, which is covered in graphene film surface, and is logical during by paraffin disengaging graphene film
Cross what solvent was dissolved, during the entire process of transfer graphene film, be used to peel off paraffin and stone without direct active force
Black alkene, and the pattern of graphene film is intactly replicated, realize the basic not damaged transfer of graphene film.Meanwhile,
Paraffin has the characteristics of low temperature melts and is water insoluble, reduces the operation difficulty of graphene film transfer, is conducive to determining
The removal technique of growth substrates.And paraffin is cheap, cost reduce further.
In an embodiment of the present invention, growth substrates include metal, alloy conductor or semiconductor.Such as, it can select
Pt, Ni, Cu, Co, Ir, Ru, Au, Ag metal and its alloy, can also select Si, SiO2、Al2O3Semiconductor or both answer
Condensation material.In an embodiment of the present invention, growth substrates are preferably Ni or Cu.
In an embodiment of the present invention, the thickness 1nm-10mm of growth substrates.The thickness of growth substrates can influence graphene
The growth conditions of film and the difficulty for shifting graphene film, in order that easily operated when must shift graphene film, therefore,
Preferably, the thickness of growth substrates is 5-100 μm.
It is that to be covered with the paraffin of fusing whole by being coated with the paraffin of fusing it should be noted that in embodiments of the invention
The surface of individual graphene film.The mode of coating include it is a variety of, for example:Topple over, be added dropwise.In other embodiments, to coating
Mode do not limit, as long as can realize cause fusing paraffin cover graphene film surface.Need explanation
It is, when the paraffin of fusing to be covered in the surface of graphene film, to avoid mechanical force on the surface of graphene as far as possible, make
Into the damage of graphene film.In addition, the paraffin of fusing can cover the whole area of graphene film, can be part face
Product, this can be determined according to the area of the graphene film finally needed to use.Moreover, in an embodiment of the present invention, stone
Black alkene film is to be grown in growth substrates surface by the method for chemical vapor deposition (CVD), is given birth to by chemical vapour deposition technique
Long graphene film, can obtain the graphene film of the single or multiple lift of large area, and resulting graphene film quality is good,
And it is easy to transfer.
In an embodiment of the present invention, it is possible to use ready-made growth has the growth substrates of graphene film, has in growth
The upper paraffin of that surface coating of graphene film;Can also be after growth substrates superficial growth graphene film, then
Graphene film surface is coated with paraffin.In addition, in an embodiment of the present invention, the growing method of graphene is also not necessarily limited to chemical gas
Phase sedimentation.
It should be noted that the operable of graphene film can be influenceed in the paraffin thickness that graphene film surface is coated with
Property, paraffin thickness is too thin, is easily broken during transfer;Paraffin thickness is too thick, and difficulty is higher when removing paraffin;Therefore, in the present invention
Embodiment in, the paraffin thickness of coating is 1 μm of -10mm, preferably 0.5-3mm.
After after paraffin solidification, remove growth substrates and obtain paraffin/graphene composite film, remove the method bag of growth substrates
Include at least one in chemical corrosion method, electrochemical erosion method and Bubbling method.Chemical corrosion method, electrification can be single use
Learn etch or Bubbling method;Can also be that chemical corrosion method and electrochemical erosion method, electrochemical erosion method and bubbling is applied in combination
Method, and chemical corrosion method and Bubbling method;Can be chemical corrosion method, the three kinds of methods combinations of electrochemical erosion method and Bubbling method again
Use.In three kinds of minimizing technologies, during removing growth substrates using chemical corrosion method, the mechanical force almost without macroscopic view
Graphenic surface is applied to, can farthest ensure the integrality of graphene film, therefore, the method for removing growth substrates
Preferably chemical corrosion method.
Remove after growth substrates, paraffin/graphene composite film is placed in into target substrate makes graphene film be served as a contrast with target
Bottom is contacted, and to target substrate heating until paraffin is fitted in target substrate, paraffin is removed using solvent.
In an embodiment of the present invention, if paraffin is not fitted with target substrate, paraffin is removed in later use solvent
When, the solvent or paraffin of liquid have tension force effect to graphene film surface, be likely to result in graphene film under tension and
It is damaged.Therefore, in an embodiment of the present invention, it is necessary to target substrate heating make paraffin soften after be fitted in target substrate,
Preferably, subsequent operation process can so be avoided until paraffin is intactly fitted in target substrate to target substrate heating
The tension force of middle liquid influences the integrality of graphene film.
Paraffin is noncrystal, and fixed fusing point, does not start fusing at 40 DEG C generally, needed always in fusion process
Heat absorption, fusing would not be continued by stopping heating paraffin wax.In order to ensure that paraffin can fully melt, therefore, in the implementation of the present invention
In example, the temperature heated to target substrate is 40-200 DEG C, and the heat time is 1-1000s.Preferably, target substrate is heated
Temperature is 50-80 DEG C, and the heat time is 10-100s., can be with when heating-up temperature is equal to or slightly exceeded the fusion temperature of paraffin
Avoid paraffin from being fused into the breakage that liquid causes graphene film in flow process rapidly, select preferred heating-up temperature and add
The hot time, it can make it that paraffin is preferably fitted with target substrate.
In addition, in the step of removing paraffin, the solvent used is organic solvent, it is preferable that solvent includes dimethylbenzene, vapour
At least one in oil, kerosene, carbon disulfide, chloroform and ethanol.Paraffin is organic matter, can preferably be dissolved in diformazan
In the organic solvents such as benzene, gasoline, kerosene, carbon disulfide, chloroform and ethanol.
A kind of preparation method of sensor, including:Channel electrode is made on graphene film surface made from the above method,
Graphene film is made to the pattern of touch sensing, encapsulates and then enters in the graphene film surface laminating optical cement of patterning
Row deaeration is handled.
Graphene film is that graphene is to possess cellular made from the method using above-mentioned new transfer graphene film
The superpower what is said or talked about compound of structure, flexible and more further conductive than silicon, the graphene film obtained using the above method is complete, basic
Lossless and area is big, therefore the graphene film can make sensor produce stronger electric signal for the making of sensor.
The feature and performance to the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of method of new transfer graphene film, including:Grown in thickness for 30 μm of copper foil surface by CVD
Graphene film.After the completion of growth, the paraffin after melting, and further heating Copper Foil lining are coated with graphene film surface
Bottom, makes paraffin be evenly distributed in copper foil surface, wherein, paraffin thickness is 2mm or so.After after paraffin solidification, pass through chemical attack
Method erodes Copper Foil substrate, and the graphene face of paraffin/graphene composite film then is placed in into silicon chip surface.In 70 DEG C of temperature strip
Heating 1min is carried out to silicon chip under part, paraffin is fitted in silicon chip surface.Then xylene soluble paraffin is used, and by Wafer Cleaning
Clean to remove paraffin completely, the so far substantially lossless transfer of graphene film is completed.
Embodiment 2
A kind of method of new transfer graphene film, including:Grown in thickness for 50 μm of nickel foil surface by CVD
Graphene film.After the completion of growth, the paraffin after melting, and further heating nickel foil lining are coated with graphene film surface
Bottom, makes paraffin uniform in nickel foil surface distributed, wherein, paraffin thickness is 1mm or so.It is rotten by electrochemistry after after paraffin solidification
Erosion method erodes nickel foil substrate, and the graphene face of paraffin/graphene composite film then is placed in into silicon chip surface.In 70 DEG C of temperature
Under the conditions of to silicon chip carry out heating 1min, paraffin is intactly fitted in silicon chip surface.Xylene soluble paraffin is then used, and will
Wafer Cleaning totally removes paraffin completely, and the so far substantially lossless transfer of graphene film is completed.
Embodiment 3
A kind of method of new transfer graphene film, including:Grown in thickness for 50 μm of copper foil surface by CVD
Graphene film.After the completion of growth, the paraffin after melting, and further heating Copper Foil lining are coated with graphene film surface
Bottom, makes paraffin be evenly distributed in copper foil surface, wherein, paraffin thickness is 1mm or so.After after paraffin solidification, shelled by Bubbling method
From Copper Foil substrate, the graphene face of paraffin/graphene composite film is then placed in silicon chip surface.It is right under 70 DEG C of temperature conditionss
Silicon chip carries out heating 1min, paraffin is intactly fitted in silicon chip surface.Paraffin then is dissolved with gasoline, and Wafer Cleaning is done
Net to remove paraffin completely, the so far substantially lossless transfer of graphene film is completed.
Embodiment 4
A kind of method of new transfer graphene film, including:Given birth in thickness for 100 μm of copper foil surface by CVD
Long graphene film.After the completion of growth, the paraffin after melting, and further heating Copper Foil lining are coated with graphene film surface
Bottom, makes paraffin be evenly distributed in copper foil surface, wherein, paraffin thickness is 3mm or so.After after paraffin solidification, pass through chemical attack
Method erodes Copper Foil substrate, and the graphene face of paraffin/graphene composite film then is placed in into silicon chip surface.In 50 DEG C of temperature strip
Heating 100s is carried out to silicon chip under part, paraffin is intactly fitted in silicon chip surface.Paraffin then is dissolved with kerosene, and by silicon chip
Clean up and remove paraffin completely, the so far substantially lossless transfer of graphene film is completed.
Embodiment 5
A kind of method of new transfer graphene film, including:Grown in thickness for 5 μm of copper foil surface by CVD
Graphene film.After the completion of growth, the paraffin after melting, and further heating Copper Foil lining are coated with graphene film surface
Bottom, makes paraffin be evenly distributed in copper foil surface, wherein, paraffin thickness is 0.5mm or so.After after paraffin solidification, by chemical rotten
Erosion method erodes Copper Foil substrate, and the graphene face of paraffin/graphene composite film then is placed in into silicon chip surface.In 80 DEG C of temperature
Under the conditions of to silicon chip carry out heating 10s, paraffin is intactly fitted in silicon chip surface.Paraffin then is dissolved with ethanol, and by silicon
Piece is cleaned up removes paraffin completely, and the so far substantially lossless transfer of graphene film is completed.
Embodiment 6
A kind of method of new transfer graphene film, including:Grown in thickness for 10mm copper foil surface by CVD
Graphene film.After the completion of growth, the paraffin after melting, and further heating Copper Foil lining are coated with graphene film surface
Bottom, makes paraffin be evenly distributed in copper foil surface, wherein, paraffin thickness is 10mm or so.After after paraffin solidification, shelled by Bubbling method
From Copper Foil substrate, the graphene face of paraffin/graphene composite film is then placed in silicon chip surface.Under 200 DEG C of temperature conditionss
Heating 1s is carried out to silicon chip, paraffin is intactly fitted in silicon chip surface.Then paraffin is dissolved with chloroform, and Wafer Cleaning is done
Net to remove paraffin completely, the so far substantially lossless transfer of graphene film is completed.
Embodiment 7
A kind of method of new transfer graphene film, including:Grown in thickness for 1nm copper foil surface by CVD
Graphene film.After the completion of growth, the paraffin after melting, and further heating Copper Foil lining are coated with graphene film surface
Bottom, makes paraffin be evenly distributed in copper foil surface, wherein, paraffin thickness is 1 μm or so.After after paraffin solidification, pass through chemical attack
Method erodes Copper Foil substrate, and the graphene face of paraffin/graphene composite film then is placed in into silicon chip surface.In 40 DEG C of temperature strip
Heating 1000s is carried out to silicon chip under part, paraffin is intactly fitted in silicon chip surface.Then paraffin is dissolved with carbon disulfide, and
Wafer Cleaning is totally removed into paraffin completely, the so far lossless transfer of basic graphene film is completed.
A kind of preparation method of sensor, including:Channel electrode is made on graphene film surface made from the above method,
Graphene film is made to the pattern of touch sensing, encapsulates and then enters in the graphene film surface laminating optical cement of patterning
Row deaeration is handled.
In summary, a kind of method of new transfer graphene film of the embodiment of the present invention and the preparation side of sensor
In method, the method for new transfer graphene film, paraffin dissolves stone as transfer medium by heating melt paraffin and solvent
Wax, it is possible to achieve substantially lossless transfer graphene film.On the one hand, it is liquid that paraffin, which is covered in graphene film surface,;Separately
On the one hand, dissolved when paraffin being departed from into graphene film by solvent, during the entire process of transfer graphene film,
There is no direct active force to be used to peel off paraffin and graphene, and intactly replicate the pattern of graphene film, realize
The substantially lossless transfer of graphene film.Meanwhile, paraffin has the characteristics of low temperature melts and is water insoluble, reduces graphene
The operation difficulty of film transfer, is conducive to determining the removal technique of growth substrates.And paraffin is cheap, it reduce further
Cost.
The preparation method of sensor, is that graphene is to possess honeybee using made from graphene film made from the above method
The superpower what is said or talked about compound of nest shape structure, it is flexible and more further conductive than silicon, the graphene film that is obtained using the above method is complete,
Basic not damaged and area is big, therefore the graphene film is used for makings of sensor can make the stronger telecommunications of sensor generation
Number.
Embodiments described above is a part of embodiment of the invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of method of new transfer graphene film, it is characterised in that including:
The paraffin of fusing is set to be covered in the surface for the graphene film for being formed at growth substrates surface;
After after paraffin solidification, remove the growth substrates and obtain paraffin/graphene composite film;
The surface that the paraffin/graphene composite film is placed in into target substrate makes the graphene film and the target substrate
Contact, to target substrate heating until the paraffin is fitted in the target substrate, the paraffin is removed using solvent.
2. the method for new transfer graphene film according to claim 1, it is characterised in that the paraffin of coating is thick
Spend for 1 μm of -10mm.
3. the method for new transfer graphene film according to claim 2, it is characterised in that the paraffin of coating is thick
Spend for 0.5-3mm.
4. the method for new transfer graphene film according to claim 1, it is characterised in that remove the growth substrates
Method include chemical corrosion method, electrochemical erosion method and Bubbling method at least one.
5. the method for new transfer graphene film according to claim 4, it is characterised in that remove the growth substrates
Method be chemical corrosion method.
6. the method for new transfer graphene film according to claim 1, it is characterised in that add to the target substrate
The temperature of heat is 40-200 DEG C, and the heat time is 1-1000s.
7. the method for new transfer graphene film according to claim 6, it is characterised in that the temperature is 50-80
DEG C, the heat time is 10-100s.
8. the method for new transfer graphene film according to claim 1, it is characterised in that the solvent is organic molten
Agent;Preferably, the solvent includes at least one in dimethylbenzene, gasoline, kerosene, carbon disulfide, chloroform and ethanol.
9. the method for new transfer graphene film according to claim 1, it is characterised in that the thickness of the growth substrates
Spend for 1nm-10mm;Preferably, the thickness of the growth substrates is 5-100 μm.
10. a kind of preparation method of sensor, it is characterised in that including:It is made in the method described in claim any one of 1-9
Graphene film surface make channel electrode, the graphene film is made to the pattern of touch sensing, in patterning
The encapsulation of graphene film surface laminating optical cement and then progress deaeration processing.
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CN107857252A (en) * | 2017-10-13 | 2018-03-30 | 浙江大学 | A kind of preparation method of independent self-supporting graphene film |
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CN108439375A (en) * | 2018-03-15 | 2018-08-24 | 浙江大学 | The method of copper foil directional etching when being shifted for graphene |
CN109133174A (en) * | 2018-08-21 | 2019-01-04 | 中国地质大学(北京) | The transfer method and two-dimensional material of two-dimensional material and its application |
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CN108439375B (en) * | 2018-03-15 | 2020-07-31 | 浙江大学 | Method for copper foil directional corrosion during graphene transfer |
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CN109133174A (en) * | 2018-08-21 | 2019-01-04 | 中国地质大学(北京) | The transfer method and two-dimensional material of two-dimensional material and its application |
CN111362258A (en) * | 2020-02-12 | 2020-07-03 | 浙江大学 | Graphene film transfer method using beeswax as supporting layer |
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CN111763923A (en) * | 2020-06-30 | 2020-10-13 | 中国科学院上海微***与信息技术研究所 | Two-dimensional material layer transfer method after preparation |
CN114229838A (en) * | 2021-12-27 | 2022-03-25 | 松山湖材料实验室 | Graphene device, multilayer film, and manufacturing method and application thereof |
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